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建立一种 LC-MS/MS 法测定头发中丙泊酚葡萄糖醛酸,初步研究剂量与头发浓度的关系。

Development of a LC-MS/MS method for determination of propofol-glucuronide in hair and preliminary study on relationships between dose and hair concentration.

机构信息

College of Pharmacy, Duksung Women's University, Seoul, South Korea; National Institute of Food and Drug Safety Evaluation, Osong, South Korea; Innovative Drug Center, Duksung Women's University, 33, Samyangro 144-gil, DobongGu, Seoul, South Korea.

College of Pharmacy, Duksung Women's University, Seoul, South Korea; Innovative Drug Center, Duksung Women's University, 33, Samyangro 144-gil, DobongGu, Seoul, South Korea.

出版信息

Forensic Sci Int. 2020 Jan;306:110070. doi: 10.1016/j.forsciint.2019.110070. Epub 2019 Nov 19.

Abstract

Propofol abuse has been reported worldwide, suggesting the need to establish analytical methods for human biological samples to investigate the abuse of propofol. This study aimed to investigate the relationship between dose and hair concentration using a simple and rapid analytical method developed and validated in this study. In the sample preparation, hair samples were washed with distilled water and methanol and extracted in methanol during 16h at room temperature. After centrifugation and evaporation, the residue was reconstituted and filtered through a 0.22μm membrane filter before LC-MS/MS analysis. The precursor-to-product ion transitions were 353 → 175, 113 for propofol glucuronide and m/z 370 → 175, 113 for internal standard(propofol glucuronide-d). The calibration curves were satisfactory (R=0.9997) and the limits of detection and quantification were 2 and 5pg/mg, respectively. In addition, this study collected the history of propofol use from subjects using a questionnaire and analyzed subjects' hair samples using a validated analytical method. As a result, the concentrations of propofol glucuronide ranged from 7 to 122pg/mg (mean : 51pg/mg). There were cases of positive relationships, but generally there was no correlation between dose and hair concentration.

摘要

丙泊酚滥用已在全球范围内得到报道,这表明有必要建立分析人生物样本的方法,以调查丙泊酚的滥用情况。本研究旨在通过建立和验证本研究中的简单快速分析方法来研究剂量与毛发浓度之间的关系。在样品制备中,先用蒸馏水和甲醇洗涤毛发样品,然后在室温下用甲醇提取 16 小时。离心和蒸发后,残渣用 0.22μm 膜过滤器重新配制并过滤,然后进行 LC-MS/MS 分析。前体到产物离子的跃迁分别为 353→175、113(丙泊酚葡萄糖醛酸苷)和 m/z370→175、113(内标丙泊酚葡萄糖醛酸苷-d)。校准曲线令人满意(R=0.9997),检测限和定量限分别为 2 和 5pg/mg。此外,本研究使用问卷收集了受试者使用丙泊酚的历史,并使用经过验证的分析方法分析了受试者的毛发样本。结果显示,丙泊酚葡萄糖醛酸苷的浓度范围为 7 至 122pg/mg(平均值:51pg/mg)。虽然有阳性关系的案例,但一般来说,剂量与毛发浓度之间没有相关性。

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